EP0621069A1 - Procédé d'adsorption pour la production d'oxygène 99+% à partir de l'air - Google Patents

Procédé d'adsorption pour la production d'oxygène 99+% à partir de l'air Download PDF

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Publication number
EP0621069A1
EP0621069A1 EP94106069A EP94106069A EP0621069A1 EP 0621069 A1 EP0621069 A1 EP 0621069A1 EP 94106069 A EP94106069 A EP 94106069A EP 94106069 A EP94106069 A EP 94106069A EP 0621069 A1 EP0621069 A1 EP 0621069A1
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EP
European Patent Office
Prior art keywords
oxygen
adsorption zone
adsorption
air
steps
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP94106069A
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German (de)
English (en)
Inventor
Shivaji Sircar
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Products and Chemicals Inc
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Air Products and Chemicals Inc
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Filing date
Publication date
Application filed by Air Products and Chemicals Inc filed Critical Air Products and Chemicals Inc
Publication of EP0621069A1 publication Critical patent/EP0621069A1/fr
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/047—Pressure swing adsorption
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02—Preparation of oxygen
    • C01B13/0229—Purification or separation processes
    • C01B13/0248—Physical processing only
    • C01B13/0259—Physical processing only by adsorption on solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/12—Oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/102—Nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40003—Methods relating to valve switching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/403—Further details for adsorption processes and devices using three beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/414—Further details for adsorption processes and devices using different types of adsorbents
    • B01D2259/4141—Further details for adsorption processes and devices using different types of adsorbents within a single bed
    • B01D2259/4145—Further details for adsorption processes and devices using different types of adsorbents within a single bed arranged in series
    • B01D2259/4146—Contiguous multilayered adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/0407—Constructional details of adsorbing systems
    • B01D53/0423—Beds in columns
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0046—Nitrogen

Definitions

  • the present invention relates to an adsorption process which uses an oxygen selective adsorbent to produce 99+% oxygen from air in a single stage operation.
  • Adsorption processes which produce oxygen from air typically rely on selective physical adsorption (equilibrium based) of nitrogen over oxygen on a zeolite based adsorbent.
  • the oxygen product is recovered as that portion of the feed air which passes through the adsorption zone.
  • a state of the art example is the process taught in US Patent 4,756,723 by Sircar.
  • the nitrogen selective adsorbents used in these processes generally do not also adsorb argon. Since the ratio of oxygen to argon in ambient air is approximately 20:1, this limits the maximum attainable purity of the oxygen product stream in a single stage operation to approximately 95%, even assuming complete nitrogen removal. A higher purity would require further processing in a second stage of operation which is typically accomplished by selective physical adsorption (kinetic based) of oxygen over argon/nitrogen on a carbon based adsorbent.
  • the adsorption zone will also contain co-adsorbed and/or void space impurities (primarily nitrogen) which reduces the purity of the oxygen product.
  • the present invention overcomes this problem and produces a 99+% oxygen product by rinsing the adsorption zone with essentially pure oxygen prior to the depressurization step in order to purge from the adsorption zone any co-adsorbed or void space impurities.
  • Rinsing the adsorption zone with the more adsorbable component prior to depressurization is taught in the art. See for example US Patent 4,077,779 and published European application 0 913 716 (both by Sircar et al) in the context of fuel gas fractionation and US Patent 4,013,429 (also by Sircar et al) in the context of air fractionation wherein nitrogen is the more adsorbable component.
  • the adsorption prior art does not teach such a pre-depressurization rinse step in the context of air fractionation wherein oxygen is the more adsorbable component.
  • the present invention is a process to produce 99+% oxygen from air in a single stage operation comprising the steps of:
  • steps (a) through (d) are performed as a continually repeating cycle of steps and are effected in a system comprising a plurality of adsorption zones which each undergo their respective cycle of steps while collectively operated sequentially in parallel with one another.
  • Figure 1 is drawing illustrating one embodiment of the present invention.
  • Figure 1 is a schematic diagram illustrating one embodiment of the present invention wherein the present invention is effected in a system comprising three adsorption zones which each undergo their respective cycle of steps (a) through (d) while collectively operated sequentially in parallel with one another.
  • Figure 1's process configuration consists of an air blower B, three adsorption columns C1, C2, and C3 each containing an oxygen selective adsorbent, vacuum compressor V, and valves 11-13, 21-23, 31-33, 41-43, 51-53, and 61.
  • Table 1 summarizes Fig. 1's valve sequence and adsorption column step sequence for one complete cycle.
  • Table I utilizes 6 time intervals and a total elapsed time of 12 time units to cover the four separate steps of the cycle so that the relative times for each step can be clearly indicated. It should be recognized that Figure 1's embodiment and the operation sequence of Table 1 is only an example. Other embodiments can be easily designed by one skilled in the art.
  • pressure swing in Figure 1 is between near ambient pressure and sub-ambient pressure
  • other pressure swings are also possible. For example, one could perform the adsorption and rinse steps at an above ambient pressure while reducing the pressure to near ambient or sub-ambient pressure during the depressurization step.
  • Figure 1 assumes that the feed air has been dried prior to its fractionation. If desired, one can integrate the drying of the feed air with the fractionation itself by placing a layer of a desiccant material at the feed ends of the columns in order to dry the air before it reaches the oxygen selective adsorbent. In such a case, the adsorbed water will be desorbed along with the oxygen product during the depressurization step and thus the oxygen product will be wet.
  • Table 1's step sequence and valve sequence will be described as it relates to the operation of Figure 1's adsorption column C1.
  • column C1 begins the adsorption step or step (a) of the present invention.
  • Ambient air is introduced into column C1 at near ambient pressure through blower B and open valve 11.
  • a nitrogen-enriched stream is withdrawn through open valve 21.
  • valve 22 is opened so that column C1's nitrogen-enriched effluent can be used to repressurize column C2 which is currently on step (d) of the present invention.
  • column C1 is nearly saturated with air and column C1's adsorption step is terminated by closing valves 11 and 21.
  • column C1 undergoes the rinse step or step (b) of the present invention.
  • column C1 is rinsed cocurrently to the feed flow with a portion of the 99+% oxygen effluent from column C3 which is currently on step (c) of the present invention.
  • the 99+% oxygen effluent from column C3 is removed through open valve 33 and is introduced into column C1 at near ambient pressure through open valves 61 and 41.
  • the effluent from this rinse step which has an air like composition, is withdrawn through open valve 51. If desired, it can be recycled to the feed air.
  • column C1 begins the depressurization step or step (c) of the present invention.
  • column C1 is desorbed and evacuated by reducing its pressure to approximately 0.08-0.3 atmospheres. This pressure reduction is accomplished by opening valve 31 and subjecting column C1 to a vacuum with vacuum compressor V. The effluent from this time interval is the 99+% oxygen product which is removed from the system as the oxygen product.
  • valves 42 and 61 are opened so that a portion of column C1's 99+% oxygen effluent can be used to rinse column C2 which is currently on step (b) of the present invention.
  • column C1 undergoes the repressurization step or step (d) of the present invention.
  • Valve 31 is closed and valves 21 is opened in order to allow nitrogen-enriched effluent from column C3, which is currently undergoing the adsorption step, to repressurize column C1 to near ambient pressure.
  • column C1's cycle is complete and a new cycle can commence.
  • Each adsorption column undergoes a similar sequence of operation as is described for column C1 as can be further detailed from Table 1.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
EP94106069A 1993-04-21 1994-04-19 Procédé d'adsorption pour la production d'oxygène 99+% à partir de l'air Withdrawn EP0621069A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US5102993A 1993-04-21 1993-04-21
US51029 1993-04-21

Publications (1)

Publication Number Publication Date
EP0621069A1 true EP0621069A1 (fr) 1994-10-26

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EP (1) EP0621069A1 (fr)
CA (1) CA2121312A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5833737A (en) * 1996-05-20 1998-11-10 Institute Of Research And Innovation Enrichment of krypton in oxygen/nitrogen mix gas
US7651549B2 (en) 2006-06-13 2010-01-26 Air Products And Chemicals, Inc. Pressure swing adsorption process with improved recovery of high-purity product
FR3006909A1 (fr) * 2013-06-18 2014-12-19 Nitrocraft Procede d'epuration d'un melange gazeux et generateur correspondant
JP2018090479A (ja) * 2016-11-30 2018-06-14 大陽日酸株式会社 窒素及び酸素の製造方法及び製造システム
WO2022046726A1 (fr) * 2020-08-24 2022-03-03 Eisenhaure David B Centrale électrique efficace utilisant une source de chaleur à haute température

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4359328A (en) * 1980-04-02 1982-11-16 Union Carbide Corporation Inverted pressure swing adsorption process
EP0121042A2 (fr) * 1983-03-07 1984-10-10 Bergwerksverband GmbH Procédé de production d'azote
US4915711A (en) * 1989-05-18 1990-04-10 Air Products And Chemicals, Inc. Adsorptive process for producing two gas streams from a gas mixture
US5135548A (en) * 1991-05-08 1992-08-04 Air Products And Chemicals, Inc. Oxygen selective desiccants

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4359328A (en) * 1980-04-02 1982-11-16 Union Carbide Corporation Inverted pressure swing adsorption process
EP0121042A2 (fr) * 1983-03-07 1984-10-10 Bergwerksverband GmbH Procédé de production d'azote
US4915711A (en) * 1989-05-18 1990-04-10 Air Products And Chemicals, Inc. Adsorptive process for producing two gas streams from a gas mixture
US5135548A (en) * 1991-05-08 1992-08-04 Air Products And Chemicals, Inc. Oxygen selective desiccants

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5833737A (en) * 1996-05-20 1998-11-10 Institute Of Research And Innovation Enrichment of krypton in oxygen/nitrogen mix gas
US7651549B2 (en) 2006-06-13 2010-01-26 Air Products And Chemicals, Inc. Pressure swing adsorption process with improved recovery of high-purity product
FR3006909A1 (fr) * 2013-06-18 2014-12-19 Nitrocraft Procede d'epuration d'un melange gazeux et generateur correspondant
EP2815798A1 (fr) * 2013-06-18 2014-12-24 Nitrocraft Procédé d'épuration d'un mélange gazeux par adsorption à variation de pression et générateur correspondant
JP2018090479A (ja) * 2016-11-30 2018-06-14 大陽日酸株式会社 窒素及び酸素の製造方法及び製造システム
WO2022046726A1 (fr) * 2020-08-24 2022-03-03 Eisenhaure David B Centrale électrique efficace utilisant une source de chaleur à haute température

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Publication number Publication date
CA2121312A1 (fr) 1994-10-22

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